Production of bromin or bromids.



P. I. DU PONT.

PRODUCTION OF BROMIN 0B BROMIDE.

APPLICATION FILED JULY 22, 1911.

Patented June 10, 1913.

2 SHEETS-SHEET 1.

HI I F n l v ln H 4 INVENTOI? AL @'LL L WITNESSES:

F. I. DU PONT.

PRODUCTION OF BROMIN 0B BROMIDS.

APPLICATION FILED JULY 22, 1911.

Patented June 10, 1913.

2 SHEETS-SHEET 2.

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m z/vroe M J 9620M ATTOR/VEVJ.

: uolns runs In, manxurno. Ilsunmtun. n

and the brine to be violently emulsified.

I the brine, is

content, if not of the desired strength, may

a citizen of the United States,

from an 'rying a sufficient-s amount of bromin for 'vessel which carries a medlum which will FRANCIS I. m1 PONT, 0F WILMINGTON, DELAWARE, nssrclxion TO INTERNATIONAL HALOID COMPANY, ACORPORATION or nnn'iwnnn.

PRODUCTION OF BROMIN 0R BROMIDS.

Specification of Letters Patent. Application filed July 22, 1911. Serial No. 639,872.

To all whom it may concern;

ing the water, the vessel Be it known that-I, FRANCIS Jected to heat sufiicient to vaporize any carbon tetra chlorid absorbed by the medium, which is then condensed and returned to t e original brine solution.

he carbon tetra chlorid containing in solution the bromin, and from which the I. DU PoNT, residing at Vilmingtoincounty of Newcastle, and State of Del haveinvented a new and useful Improvement in the Production of Bromin or Bromids, of which the following is a full, clear, and exact description, reference being had to the accompanying drawings, which for a part of this specification.

M invention relates to a method or process l hr the production of bromids or bromin, particularly anhydrous bromids, such as anhydrous antimony bromid. In my process this bromid or bromin is produced aqueous solution, for instance, brine, containing the usual small content of combined bromin. v

In my process the solution, say brine, is first electrolyzed, or otherwise treated to set free the An example of the from desired to combine with the r in, for instance, powdered metallic an tiiony, if it is desired to use the process to 1 ake antimony bromid. The rotation of the agitators in the vessel causes the combining element, for instance antimony, to combine with the bromin dissolved in the carbon tetra chlorid, and bromid of antithe agitation is stopped, and bottom it may be removed. the first mentioned which the carbon tetra I bromin was sepa rated, is passed into a second vessel which is heated, and which drives off the bromin extracting agent and any carried bromin. This may be c ndensed, and if rweak, returned to the oiiginal brine solution, or if strong enough, may be carried to the vessel in which the calcium chlorid is used, and from is passed to the agitating. vessel in which it is combined with the antimony. e brine remaining after the action in the Dow, April 12, 1892. In my process I add to such solution, say brine, a bromin extracting reagent, for instance, carbon tetra chlorid, and agitate such reagent in the rine. This causes the carbon tetra chlorid' The bromin, or a certain part of it from extracted by the bromin extracting reagent, for instance, carbon tetra 'd, and remains with this carbon tetra The emulsion, is then separated in a vessel, which allows the carbon tetra chlorid with its carried bromin, to fall to the bottom of the vessel from which it can be readily delivered.

The carbon tetra chlorid, with its bromin waste, it still contains sufficient bromin, it maybe returned to t e original brine solution.

If it is desired to use the process in the production of bromin, then the vessel in which the antimony or other combining elements is added to bromin is not used, nor is be conveyedbaclg to the original brine solution, or if it is of the desired strength, carfurther action, it

absorb the water. Y

of bromin, and the bromin extracting reagent, carbon tetra chlorid, substantially ime from water. The water extracting medium, for instance, calcium chlorid, may be revivified by removing it from the vessel and extracting :the Water. Before remov ing this medium from the vessel, or extract.-

being used to produce bromin in desiccating the carbon tetra chlorid solution of Therefore, in such cases, the vessels in which calcium chlorid is used can be dispensed with.

Patented Juine 10, 1913.

should be subing the bromin aqueous solutions, 1n a free condition ity for bromin 1consists in doing aqueous solution and The carbon tetra chlorid solutioncarrying the bromin which has been extracted, is'subjected to a .fractional distillation whereby.

step of separating the extracting liquid by gravity from 1t may include the aqueous solution. Further, the step of drying or freeing from water thebromin when in solution in the extracting liquid.

I other substance of which it is desired to produce a bromidrwhile still in solution in the extracting liquid. I

I will now describe an apparatus bywhich my invention may be carried out.

Figure I represents a general view of an apparatus for carrying out my invention.

connected to the shaft 0, rotated by pulley d.

the separator a pipe. 3

Fig. 2 shows another form of apparatus for carrying out my invention. Fig. 3 shows another general view of an apparatus for carrying out my invention.

a is. a vessel containing the agitators b which shaft ads 6 is the inlet pipe previously been treated to produce bromin in a free condition, and f is an inlet for the bromin extracting liquid, which may be, for

.- instance, carbon tetra chlorid.

g represents the level of the brine.

From the vessel a a pipe it passes to a separator i, and from the upper portion of "passes to the steam jacketed vessel k, which vessel has the trap outlet 1. v

m [is a pipe leading from the lower portion of vessel'i and enteringinto pipe n. This. pipe at has the valve 200.; On the top of the steam jacketed vessel It a pipe 0 leads to the condenser 11 and fromjthe. condenser p a pipe 13 leads to the pipe n? The pipe n terminates in the vessel 0... The pipe n has the valve 201. It has the branch pipe 8 terminating in the pipe 9, the ends of which pipe-9 enter-,respectwely' the steam jacketed vessels g and 1'. On the pipe 9 are the valves ,9. From the top of these vessels 4 and 1' are pipes t, having valves M, which connect with the pipe '11, which pipe v terminates n the pipe 0. The lower portion of the vessels 9 and 1 have outlets controlled by the valves tends to the jacketed vessel 1 agitators 2 on. the. shaft 1. 2 an' outlet this with the intermediate v Finally, it consists in causing the bromin to act upon a metal or for the brinewhich has to be vaporized, and

passes back sel a.

which is not injured by water,

connecting with the pipe :1; which exhaving the .from vessel 3/ controlled by valve 3 and 15 is a steam pipe for the jacket of vessel y controlled by the valve 16.

4 are steam pipes for the vessels g and 1, controlled by the alves 5.

6 is a valve co. trol for the jacket of thevessel 1:, .and 7 arethe valves controlling condenser p.

In operation the-brine is pumped through the pipe e into. the vessel :1 and the agitators operated. The bromin extracting reagent, say carbon tetra chlorid, is initially admitted through the inlet By the opera tion' of the'agitators an emulsion is formed in the vessel a in which emulsion the carbon tetra chlorid carries the bromin. The brine solution with the carbon tetra chlorid carrying the bromin passes into'the separator i where a large part of the carbon tetra chlorid with the carried bromin drops to the bottom. If the last mentioned solution is of sufiicient bromin strength to enable a substantial extraction of the bromin, the valves 8 are open so as to allow the car bon tetra chlorid carrying the bromin to pass into the vessels 1' and g which contain calcium chlorid or other water absorbing medium. After the Water has been absorbed the calcium chlorid, the carbon tetra chlorid carrying the bromin passes into the vessel 1/ where it is agitated in the presence of antimony. After the antimony is combined with the bromin, it will form anti mony bromidand drop to the bottom and may be removed by opening the valve 3. Sufiicient heat is applied to the jacket of this vessel to cause the carbon tetra chlorid it passes through the pipe 10 to condenser 11, from which it passes back again into the tank a through the pipe 12. I

If the carbon tetra chlorid produced with the bromin is not rich enough in bromin, tov enable a substantial extraction of bromin the valves 8 are closed, which causes this. material to returnto the original brine'solution near the bottom of the tank a. Thebrine, which is at the upper portion ofthe-tank 71 passes through the, pipe to the vessel is, where it is subjected to heat whiehdrives off the carbon tetra chlorid and its carried bromin, which is condensed in the condenser 79 and passes back through the pipe 13, and if the valves s'are open, it passes to the vessels q and 1', and if the valves 8 are closed it through the pipe n to the ves- If it is des'ired to manufacture'a bromid the vessels 9 and 1' arernot used and the pipe 8 carried directly to the'.vessel y. The plpe 8 is then providedwith a stop. cockra'nd thecarbon tetra chloii'd containing bromin, not however absolutel r-free fi-oinmoisture, is al- "lowed to enter theve ssel '1} in whatever ouaning points.

the metal, or base,

distillation and the carbon tetra chlorid returned to the system.

The covers ofthe vessels 1- and gare removable so that the calcium chlorid may be removed and rei'ivified, before such removal, however, the vessel should be heated so as to vaporize any carbon tetra chlorid and bromin in the calcium chlorid which will pass .up through the pipe 1; to the condenser p where it is condensed and either returned back to the vessels 9 and 1' for further action or' to the tank a. I

Having now fully described my invention, what I claim and desire to protect by Letters Patent is:

1. The hereinbefore described process, which consists in adding to and agitating with an aqueous solution containing uncombined bromin, a liquid substantially insoluble in the aqueous solution, and having a Copies of this patent may be obtained for five cents each, by addressingthe the bromin greater avidity for bromin than said solution, and separating the liquid containing from the aqueous layer, and a itating said bromin containing liquid with antimony.

2. The hereinbefore described process, which consists in adding to and agitating with an aqueous solution containing uncombined bromin, a liquid substantially insolub le' in the aqueous solution, and having a .greater avidity for bromin than said solution, and separating the liquid containing "the bromin from aqueous layer, and subjecting the bromin containing liquid to a drying or water removing action and then agltatlng it with antimony.

3. The hereinbefore described process, which consists in adding toand agitating with an aqueous solution containing uncombined bro-min, carbon tetra chlorid, and separating the carbon tetra chlorid with its dissolved bromin from the aqueous layer,

and causing the bromin while still in solution in the carbon tetra chlorid to act upon antimony.

In testimony of which invention, I have hereunto set my hand, at Philadelphia, on this 21st day of July, 1911.

FRANCIS I. DU PONT.

Witnesses:

M. M. HAMILTON, E. E. WALL.

Commissioner of Patent-s,

Washington, D. 0. 

